CN101334504A - Method for manufacturing erbium-doped hybrid SiO2 optical waveguides amplifier by ultraviolet light direct-writing - Google Patents
Method for manufacturing erbium-doped hybrid SiO2 optical waveguides amplifier by ultraviolet light direct-writing Download PDFInfo
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- CN101334504A CN101334504A CNA2007101180069A CN200710118006A CN101334504A CN 101334504 A CN101334504 A CN 101334504A CN A2007101180069 A CNA2007101180069 A CN A2007101180069A CN 200710118006 A CN200710118006 A CN 200710118006A CN 101334504 A CN101334504 A CN 101334504A
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Abstract
The invention provides a method used for preparing erbium-doped hybridization SiO2 optical waveguide amplifier by direct writing of ultraviolet. The method of the invention is characterized by comprising the steps as follows: step 1: a thermal oxidation method is used for generating a lower wrapping layer on a single-crystal Si underlay; step 2: an organic/inorganic hybridized sol-gel method is used to prepare the erbium-doped photosensitive SiO2 material; step 3: the photosensitive hybridized SiO2 film is rotatablely coated on the lower wrapping layer and taken as a core layer; step 4: front baking and solidifying operations are carried out; step 5: the exposure is carried out by using the ultraviolet to pass through a mask; device patterns are directly copied to the core layer; step 6: developing and rear baking operations are carried out so as to obtain the bar-shaped erbium-doped waveguide amplifier.
Description
Technical field
The invention belongs to the method for making of a kind of optical communication technique field optical amplifier, particularly a kind of ultraviolet light direct-writing is made erbium-doped hybrid SiO
2The method of optical waveguides amplifier.
Background technology
Erbium-doped optical waveguide amplifier (EDWA) is because its inner erbium ion Er
3+Energy level
4I
13/2→
4I
15/2Induced transition can be amplified the light signal of communication wavelengths 1.55 mu m ranges, and has compact optical waveguide structure, size is little, integrability, and it is integrated to be easy to realize that photoelectricity mixes, therefore obtained paying close attention to widely and studying, and be applied to optical communication field, had bright development prospect.
The making of erbium-doped optical waveguide amplifier is the SiO that at first grows on the Si substrate at present
2Under-clad layer, and then with flame hydrolysis (FHD), plasma enhanced chemical vapor deposition method (PECVD), sol-gel methods such as (sol-gel) growth waveguide core layer and erbium doped, core material commonly used is Si, SiO
2, Al
2O
3Deng III and IV family material, SiO wherein
2Have the intrinsic loss low, cheap, with the under-clad layer Perfect Matchings, and with advantages such as the compatibility of quartz glass telecommunication optical fiber is good, become the er-doped host material of widespread usage.In order to make the well restriction propagation in waveguide of light wave pattern, sandwich layer SiO
2Should have high index-contrast with upper and lower covering, and high index-contrast can realize little curved waveguide radius, make the waveguide device structure compact more, therefore will be to sandwich layer SiO
2Mix, improve its refractive index.PECVD and FHD can adjust film refractive index by mix impurity such as phosphorus and germanium in deposition process, but manufacture craft needs expensive equipment and complicated production run.Sol-gel process has that technology is simple, easy-to-use, inexpensive, material purity is high, the gained material homogeneity is good, heat treatment temperature is low, be easy to advantages such as doping, can be widely applicable in various smooth function films and the slab guide preparation, erbium ion also is easy to mixing in the waveguide material of even and high concentration.Yet traditional sol-gel process is difficult to the SiO that acquisition meets the device required thickness and do not have be full of cracks
2Film, the preparation technology that repeatedly films-anneal can cause occurring defectives such as spot, pickup on the film, influences the quality of waveguide, increases device loss.
The typical manufacture craft of existing optical waveguides amplifier is: make through series of process such as figure mask, photoetching, development and reactive ion etchings on sandwich layer, this complex technical process, apparatus expensive, production cost height, efficient are low, are not suitable for large-scale batch process.
Summary of the invention
The objective of the invention is to overcome the deficiency that background technology exists, provide a kind of ultraviolet light direct-writing to make erbium-doped hybrid SiO
2The method of optical waveguides amplifier, this method can disposable acquisition satisfy requirement on devices thickness and refractive index evenly and high concentration er-doped SiO
2Core material does not re-use expensive equipment and loaded down with trivial details etching technics.
Technical scheme of the present invention is:
The invention provides a kind of ultraviolet light direct-writing and make erbium-doped hybrid SiO
2The method of optical waveguides amplifier is characterized in that, comprises the steps:
Step 1: earlier with the thermal oxidation method under-clad layer of on the single crystalline Si substrate, growing;
Step 2: utilize the sol-gel process of hybrid to prepare er-doped photosensitivity SiO
2Material;
Step 3: spin coating photosensitivity hydridization SiO on under-clad layer
2Film is as sandwich layer;
Step 4: preceding baking, solidify;
Step 5: utilize ultraviolet light to expose then, directly copy to component graphics on the sandwich layer by mask;
Step 6: development, back baking obtain the bar shaped Erbium Doped Waveguide Amplifier.
Wherein the thickness of under-clad layer is 10 microns-20 microns SiO
2
Photosensitivity hydridization SiO wherein
2Film is photosensitivity SiO
2Material.
Hybrid er-doped photosensitivity SiO wherein
2The preparation of material, be as the first body of reaction with methyl allyl acyloxypropyl trimethoxysilane, hydrochloric acid solution is a catalyzer, mix and stir hydrolysis, mix zirconium-n-propylate and regulate refractive index, erbium nitrate solution provides erbium ion, and n-propanol is a solvent, mix 1-hydroxyl-cyclohexyl benzophenone and make material have photosensitivity, filter under the lucifuge condition and wear out into colloid.
Wherein ultraviolet light is by covering photosensitivity hydridization SiO
2The mask that is carved with the waveguide figure on the film exposes, and the film that is exposed under the mask light transmission part is further entered in organic network owing to metal zirconium, and refractive index is increased; Unexposed part refractive index is constant; Mix the photosensitivity SiO of photosensitizer 1-hydroxyl-cyclohexyl benzophenone
2Material is a kind of negativity photosensitive material, is developer with n-propanol, and the unexposed part of film will be removed through developing, and the film that is exposed can stay, and forms slab waveguide, thereby makes the bar shaped Erbium Doped Waveguide Amplifier.
After wherein developing, 300 ℃-500 ℃ back baking processing down, make the refractive index of material further improve, waveguide core layer and under-clad layer refringence are bigger, make the light wave pattern better be limited in the slab waveguide; Can activate erbium ion, improve photoluminescence intensity; Further residual solvent levels in the film that is exposed is dropped to minimumly, it is minimum to make device loss drop to.
Wherein the refractive index of waveguide core layer is to control by regulating the zirconium-n-propylate doping, and uv-exposure time, back baking temperature and time refractive index are done further adjusting; Controlled by consumption, spin coating speed, the spin coating time realization film thickness of regulating the organic solvent n-propanol, and once be coated with the thickness requirement that can reach device practicability; By regulating the erbium nitrate doping, can realize even and different concentration of Er, to obtain maximum luminous intensity.
The present invention compares with background technology, and material preparation process is simple, can adjust the thickness and the refractive index of waveguide core layer very easily, obtains uniform doping, and variable concentrations er-doped light-emitting film, reaches the designing requirement of orthoron spare; With common ultraviolet photoetching technology, can directly produce the ridge optical waveguide amplifying device, saved the SiO of equipment, complex process
2Dry etch process save cost, and heat treatment temperature is low, is suitable for large scale integration production.
Description of drawings
For further specifying concrete technology contents of the present invention, below in conjunction with embodiment and accompanying drawing describes in detail as after, wherein:
Fig. 1 a is the gluing process; Fig. 1 b is the whirl coating film forming procedure.
Fig. 2 is a contact ultraviolet photoetching synoptic diagram;
Fig. 3 is exposure back variations in refractive index synoptic diagram;
Fig. 4 is a bar shaped Erbium Doped Waveguide Amplifier diagrammatic cross-section.
Embodiment
It is described to see also Fig. 2-Fig. 4, and a kind of ultraviolet light direct-writing of the present invention is made erbium-doped hybrid SiO
2The method of optical waveguides amplifier comprises the steps:
Step 1: earlier with the thermal oxidation method under-clad layer 9 of growing on single crystalline Si substrate 10, the thickness of this under-clad layer 9 is 10 microns-20 microns SiO
2
Step 2: utilize the sol-gel process of hybrid to prepare er-doped photosensitivity SiO
2Material; This hybrid er-doped photosensitivity SiO
2The preparation of material, be as the first body of reaction with methyl allyl acyloxypropyl trimethoxysilane, hydrochloric acid solution is a catalyzer, mix and stir hydrolysis, mix zirconium-n-propylate and regulate refractive index, erbium nitrate solution provides erbium ion, and n-propanol is a solvent, mix 1-hydroxyl-cyclohexyl benzophenone and make material have photosensitivity, filter under the lucifuge condition and wear out into colloid;
Step 3: spin coating photosensitivity hydridization SiO on under-clad layer 9
2 Film 8 is as sandwich layer, this photosensitivity hydridization SiO
2Film 8 is photosensitivity SiO
2Material;
Step 4: preceding baking, solidify;
Step 5: utilize ultraviolet light 6 to expose then, directly copy to component graphics on the sandwich layer by mask 7; This ultraviolet light 6 is by covering photosensitivity hydridization SiO
2The mask that is carved with the waveguide figure 7 on the film 8 exposes, and the film that is exposed 11 under mask 7 light transmission parts is further entered in organic network owing to metal zirconium, and refractive index is increased; Unexposed part 12 refractive indexes are constant; Mix the photosensitivity SiO of photosensitizer 1-hydroxyl-cyclohexyl benzophenone
2Material is a kind of negativity photosensitive material, is developer with n-propanol, and the unexposed part 12 of film will be removed through developing, and the film 11 that is exposed can stay, and forms slab waveguide 13, thereby makes the bar shaped Erbium Doped Waveguide Amplifier;
Step 6: development, back baking obtain the bar shaped Erbium Doped Waveguide Amplifier.
After wherein developing, 300 ℃-500 ℃ back baking processing down, make the refractive index of material further improve, waveguide core layer and under-clad layer 9 refringences are bigger, and the light wave pattern better is limited in the slab waveguide 13; Can activate erbium ion, improve photoluminescence intensity; Further residual solvent levels in the film 11 that is exposed is dropped to minimumly, it is minimum to make device loss drop to.
Wherein the refractive index of waveguide core layer is to control by regulating the zirconium-n-propylate doping, and uv-exposure time, back baking temperature and time refractive index are done further adjusting; Controlled by consumption, spin coating speed, the spin coating time realization film thickness of regulating the organic solvent n-propanol, and once be coated with the thickness requirement that can reach device practicability; By regulating the erbium nitrate doping, can realize even and different concentration of Er, to obtain maximum luminous intensity.
Please consult Fig. 2 and shown in Figure 3 again, ultraviolet light direct-writing of the present invention is made erbium-doped hybrid SiO
2The method of optical waveguides amplifier comprises the steps:
(1) on single crystalline Si substrate 10, utilizes the grow SiO of 18 μ m of thermal oxidation method
2Under-clad layer 9, utilizing the prism-coupled instrument to record refractive index is 1.458 (the test wavelength is 632.8nm);
(2) colloidal sol is synthetic: get first body methyl allyl acyloxypropyl trimethoxysilane of a certain proportion of reaction (MAPTMS) and catalyzer hydrochloric acid (HCl) solution, magnetic agitation 2h hydrolysis; Then according to the requirement of necessary waveguide sandwich layer, with a certain amount of bonding agent methacrylic acid (MAA), regulate refraction materials zirconium-n-propylate (ZPO), and erbium nitrate Er (NO
3)
3Solution is magnetic agitation 30min in n-propanol (n-Propyl alcohol), mixes with hydrolysate subsequently and continues to stir 1h; Under the lucifuge condition, will stir 30min in a certain amount of photosensitizer 1-hydroxyl-cyclohexyl benzophenone (HCPK) adding colloidal sol, will place aging 24h with 0.5 μ m filtering with microporous membrane under whole colloidal sol lucifuge condition at last, the ZPO doping is many more, photosensitivity SiO
2The refractive index of material is just big more.Whole experiment is carried out at normal temperatures;
(3) gluing (consulting Fig. 1 a and Fig. 1 b): utilize the sol evenning machine spin-coating film, at first connecting pump below the vacuum tube 4 vacuumizes, tightly be adsorbed on substrate 2 on the universal stage, spinner 3 low speed or do not rotate when beginning to drip colloidal sol 1, colloidal sol 1 is dropped on the substrate 2 uniformly, rotates 3 high speed rotating afterwards, and spin coating speed is 3000rpm, time is 30s, on the substrate 2 several gel films 5 to tens micron thickness;
(4) preceding baking: for cured film, sticking version phenomenon takes place when preventing contact exposure, 100 ℃-120 ℃ preceding down baking 10min-30min, gel film 5 becomes solid-state photosensitivity hydridization SiO by original liquid state
2Film 8;
(5) ultraviolet writes: utilize the mask 7 that is carved with the waveguide figure, carry out ultraviolet light 6 exposures, ultraviolet light 6 wavelength≤365nm, power 〉=350w, time shutter 5min-30min by the contact exposure system.The film that is exposed 11 under mask 7 light transmission parts, because metal zirconium further enters in organic network, refractive index increases, refractive index increases along with the increase of time shutter, is tending towards saturated at last; Unexposed part 12 refractive indexes are constant;
(6) develop (consulting Fig. 4): the photosensitivity hydridization SiO that mixes photosensitizer HCPK
2 Film 8 is a kind of negativity photosensitive materials, and unexposed part 12 is developed and will be removed, and the film 11 that is exposed can stay, n-propanol is a developer, and development 3min-5min dries up with nitrogen afterwards, form slab waveguide 13, thereby make the bar shaped Erbium Doped Waveguide Amplifier;
(7) back baking: baking 2h in back under 300 ℃ of-500 ℃ of temperature, further improve the refractive index of slab waveguide 13, and the baking refractive index that causes in back increases effect and increases effect apparently higher than the refractive index that uv-exposure causes, this better is limited in the slab waveguide 13 the light wave pattern; Activate Er simultaneously
3+Ion improves photoluminescence intensity; And residual solvent levels in the slab waveguide 13 is reduced, make device loss reduce.
Claims (7)
1, a kind of ultraviolet light direct-writing is made erbium-doped hybrid SiO
2The method of optical waveguides amplifier is characterized in that, comprises the steps:
Step 1: earlier with the thermal oxidation method under-clad layer of on the single crystalline Si substrate, growing;
Step 2: utilize the sol-gel process of hybrid to prepare er-doped photosensitivity SiO
2Material;
Step 3: spin coating photosensitivity hydridization SiO on under-clad layer
2Film is as sandwich layer;
Step 4: preceding baking, solidify;
Step 5: utilize ultraviolet light to expose then, directly copy to component graphics on the sandwich layer by mask;
Step 6: development, back baking obtain the bar shaped Erbium Doped Waveguide Amplifier.
2, a kind of ultraviolet light direct-writing according to claim 1 is made erbium-doped hybrid SiO
2The method of optical waveguides amplifier is characterized in that, wherein the thickness of under-clad layer is 10 microns-20 microns SiO
2
3, a kind of ultraviolet light direct-writing according to claim 1 is made erbium-doped hybrid SiO
2The method of optical waveguides amplifier is characterized in that, wherein photosensitivity hydridization SiO
2Film is photosensitivity SiO
2Material.
4, a kind of ultraviolet light direct-writing according to claim 1 is made erbium-doped hybrid SiO
2The method of optical waveguides amplifier is characterized in that, wherein hybrid er-doped photosensitivity SiO
2The preparation of material, be as the first body of reaction with methyl allyl acyloxypropyl trimethoxysilane, hydrochloric acid solution is a catalyzer, mix and stir hydrolysis, mix zirconium-n-propylate and regulate refractive index, erbium nitrate solution provides erbium ion, and n-propanol is a solvent, mix 1-hydroxyl-cyclohexyl benzophenone and make material have photosensitivity, filter under the lucifuge condition and wear out into colloid.
5, a kind of ultraviolet light direct-writing according to claim 1 is made erbium-doped hybrid SiO
2The method of optical waveguides amplifier is characterized in that, wherein ultraviolet light is by covering photosensitivity hydridization SiO
2The mask that is carved with the waveguide figure on the film exposes, and the film that is exposed under the mask light transmission part is further entered in organic network owing to metal zirconium, and refractive index is increased; Unexposed part refractive index is constant; Mix the photosensitivity SiO of photosensitizer 1-hydroxyl-cyclohexyl benzophenone
2Material is a kind of negativity photosensitive material, is developer with n-propanol, and the unexposed part of film will be removed through developing, and the film that is exposed can stay, and forms slab waveguide, thereby makes the bar shaped Erbium Doped Waveguide Amplifier.
6, a kind of ultraviolet light direct-writing according to claim 1 is made erbium-doped hybrid SiO
2The method of optical waveguides amplifier is characterized in that, after wherein developing, 300 ℃-500 ℃ back baking processing down, makes the refractive index of material further improve, and waveguide core layer and under-clad layer refringence are bigger, make the light wave pattern better be limited in the slab waveguide; Can activate erbium ion, improve photoluminescence intensity; Further residual solvent levels in the film that is exposed is dropped to minimumly, it is minimum to make device loss drop to.
7, a kind of ultraviolet light direct-writing according to claim 1 is made erbium-doped hybrid SiO
2The method of optical waveguides amplifier is characterized in that, wherein the refractive index of waveguide core layer is to control by regulating the zirconium-n-propylate doping, and uv-exposure time, back baking temperature and time refractive index are done further adjusting; Controlled by consumption, spin coating speed, the spin coating time realization film thickness of regulating the organic solvent n-propanol, and once be coated with the thickness requirement that can reach device practicability; By regulating the erbium nitrate doping, can realize even and different concentration of Er, to obtain maximum luminous intensity.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101180069A CN101334504A (en) | 2007-06-27 | 2007-06-27 | Method for manufacturing erbium-doped hybrid SiO2 optical waveguides amplifier by ultraviolet light direct-writing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101180069A CN101334504A (en) | 2007-06-27 | 2007-06-27 | Method for manufacturing erbium-doped hybrid SiO2 optical waveguides amplifier by ultraviolet light direct-writing |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102289036A (en) * | 2011-08-22 | 2011-12-21 | 博创科技股份有限公司 | Method for preparing plane optical waveguide chip |
| CN104133270A (en) * | 2014-07-18 | 2014-11-05 | 南京大学 | On-chip tunable optical isolator based on active-passive optical micro cavity coupling system |
| WO2016180051A1 (en) * | 2015-05-08 | 2016-11-17 | 中兴通讯股份有限公司 | Optical waveguide preparation method and device |
| CN107099188A (en) * | 2017-06-09 | 2017-08-29 | 浙江银鹿新材料有限公司 | A kind of snowflake printing ink of toughened antiwear and preparation method thereof |
| CN114779399A (en) * | 2022-03-23 | 2022-07-22 | 吉林大学 | Method for manufacturing surface straight light waveguide |
-
2007
- 2007-06-27 CN CNA2007101180069A patent/CN101334504A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102289036A (en) * | 2011-08-22 | 2011-12-21 | 博创科技股份有限公司 | Method for preparing plane optical waveguide chip |
| CN104133270A (en) * | 2014-07-18 | 2014-11-05 | 南京大学 | On-chip tunable optical isolator based on active-passive optical micro cavity coupling system |
| CN104133270B (en) * | 2014-07-18 | 2019-08-06 | 南京大学 | On piece tunable optical isolator based on active-passive optical microcavity coupling system |
| WO2016180051A1 (en) * | 2015-05-08 | 2016-11-17 | 中兴通讯股份有限公司 | Optical waveguide preparation method and device |
| CN107099188A (en) * | 2017-06-09 | 2017-08-29 | 浙江银鹿新材料有限公司 | A kind of snowflake printing ink of toughened antiwear and preparation method thereof |
| CN114779399A (en) * | 2022-03-23 | 2022-07-22 | 吉林大学 | Method for manufacturing surface straight light waveguide |
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Open date: 20081231 |